#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 10 _journal_issue 2 _journal_year 2019 _journal_page_first 171 _journal_page_last 174 #=============================================================================== data_NifosfCO _audit_creation_method 'SHELXL-2017/1' _shelx_SHELXL_version_number '2017/1' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H28 Ni O2 P2 S2' _chemical_formula_weight 749.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.539(2) _cell_length_b 11.811(2) _cell_length_c 15.994(3) _cell_angle_alpha 83.93(3) _cell_angle_beta 88.18(3) _cell_angle_gamma 65.24(3) _cell_volume 1797.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 9879 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 31.98 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_F_000 772 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_absorpt_coefficient_mu 0.781 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_absorpt_special_details ? _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22744 _diffrn_reflns_av_unetI/netI 0.0215 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.280 _diffrn_reflns_theta_max 32.363 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.920 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.920 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.920 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 11837 _reflns_number_gt 8977 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'SAINT' _computing_structure_solution 'SIR-97' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.3190P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11837 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.51191(19) 0.44722(18) 0.73579(11) 0.0509(4) Uani 1 1 d . . . . . C2 C 0.2203(2) 0.55983(18) 0.66717(12) 0.0533(4) Uani 1 1 d . . . . . C3 C 0.41493(15) 0.12859(14) 0.66308(9) 0.0369(3) Uani 1 1 d . . . . . C4 C 0.45757(16) 0.05999(14) 0.73921(9) 0.0373(3) Uani 1 1 d . . . . . C5 C 0.41594(18) -0.04212(15) 0.75234(10) 0.0434(3) Uani 1 1 d . . . . . C6 C 0.4378(2) -0.12853(18) 0.82318(12) 0.0560(4) Uani 1 1 d . . . . . H6 H 0.490456 -0.128279 0.868673 0.067 Uiso 1 1 calc R U . . . C7 C 0.3803(3) -0.2139(2) 0.82462(15) 0.0692(6) Uani 1 1 d . . . . . H7 H 0.395492 -0.272487 0.871167 0.083 Uiso 1 1 calc R U . . . C8 C 0.3000(3) -0.2137(2) 0.75757(15) 0.0718(6) Uani 1 1 d . . . . . H8 H 0.260320 -0.271104 0.760720 0.086 Uiso 1 1 calc R U . . . C9 C 0.2776(2) -0.13137(19) 0.68690(14) 0.0611(5) Uani 1 1 d . . . . . H9 H 0.224673 -0.132916 0.641952 0.073 Uiso 1 1 calc R U . . . C10 C 0.33668(19) -0.04464(16) 0.68420(11) 0.0468(4) Uani 1 1 d . . . . . C11 C 0.47027(17) 0.18852(15) 0.85099(9) 0.0382(3) Uani 1 1 d . . . . . C12 C 0.53105(16) 0.08659(14) 0.80665(9) 0.0384(3) Uani 1 1 d . . . . . C13 C 0.67017(18) 0.00372(16) 0.83632(11) 0.0449(3) Uani 1 1 d . . . . . C14 C 0.7652(2) -0.10709(19) 0.80567(14) 0.0614(5) Uani 1 1 d . . . . . H14 H 0.740914 -0.138056 0.760589 0.074 Uiso 1 1 calc R U . . . C15 C 0.8955(2) -0.1696(2) 0.84354(19) 0.0782(7) Uani 1 1 d . . . . . H15 H 0.958906 -0.243295 0.823578 0.094 Uiso 1 1 calc R U . . . C16 C 0.9337(3) -0.1249(3) 0.91044(19) 0.0848(8) Uani 1 1 d . . . . . H16 H 1.022090 -0.169192 0.934846 0.102 Uiso 1 1 calc R U . . . C17 C 0.8433(2) -0.0166(2) 0.94122(15) 0.0712(6) Uani 1 1 d . . . . . H17 H 0.869212 0.013250 0.986305 0.085 Uiso 1 1 calc R U . . . C18 C 0.7112(2) 0.04846(18) 0.90343(11) 0.0513(4) Uani 1 1 d . . . . . C111 C 0.62276(17) 0.21075(19) 0.59907(10) 0.0490(4) Uani 1 1 d . . . . . C112 C 0.7117(2) 0.0854(3) 0.60469(15) 0.0751(7) Uani 1 1 d . . . . . H112 H 0.677210 0.025254 0.618972 0.090 Uiso 1 1 calc R U . . . C113 C 0.8533(3) 0.0488(4) 0.5889(2) 0.1112(12) Uani 1 1 d . . . . . H113 H 0.913623 -0.035875 0.594535 0.133 Uiso 1 1 calc R U . . . C114 C 0.9044(3) 0.1350(5) 0.5656(2) 0.1225(15) Uani 1 1 d . . . . . H114 H 0.999171 0.109125 0.554871 0.147 Uiso 1 1 calc R U . . . C115 C 0.8178(3) 0.2592(4) 0.55773(18) 0.1021(11) Uani 1 1 d . . . . . H115 H 0.853378 0.317870 0.540872 0.123 Uiso 1 1 calc R U . . . C116 C 0.6757(2) 0.2993(3) 0.57481(14) 0.0699(6) Uani 1 1 d . . . . . H116 H 0.616839 0.384327 0.570044 0.084 Uiso 1 1 calc R U . . . C121 C 0.35180(17) 0.30478(15) 0.52106(9) 0.0402(3) Uani 1 1 d . . . . . C122 C 0.4236(2) 0.2766(2) 0.44693(11) 0.0585(5) Uani 1 1 d . . . . . H122 H 0.520767 0.240878 0.447897 0.070 Uiso 1 1 calc R U . . . C123 C 0.3522(3) 0.3010(2) 0.37074(12) 0.0725(6) Uani 1 1 d . . . . . H123 H 0.401690 0.282941 0.321090 0.087 Uiso 1 1 calc R U . . . C124 C 0.2098(3) 0.3513(2) 0.36872(13) 0.0750(7) Uani 1 1 d . . . . . H124 H 0.162179 0.367168 0.317824 0.090 Uiso 1 1 calc R U . . . C125 C 0.1366(2) 0.3786(2) 0.44250(15) 0.0797(7) Uani 1 1 d . . . . . H125 H 0.039561 0.411594 0.441341 0.096 Uiso 1 1 calc R U . . . C126 C 0.2070(2) 0.3572(2) 0.51807(12) 0.0615(5) Uani 1 1 d . . . . . H126 H 0.156851 0.378204 0.567267 0.074 Uiso 1 1 calc R U . . . C211 C 0.17565(17) 0.27541(16) 0.81215(9) 0.0415(3) Uani 1 1 d . . . . . C212 C 0.06520(19) 0.34841(19) 0.75755(12) 0.0528(4) Uani 1 1 d . . . . . H212 H 0.063015 0.422077 0.729088 0.063 Uiso 1 1 calc R U . . . C213 C -0.0419(2) 0.3128(3) 0.74493(14) 0.0680(6) Uani 1 1 d . . . . . H213 H -0.116641 0.363537 0.709288 0.082 Uiso 1 1 calc R U . . . C214 C -0.0377(2) 0.2029(3) 0.78498(14) 0.0708(6) Uani 1 1 d . . . . . H214 H -0.108644 0.178275 0.775688 0.085 Uiso 1 1 calc R U . . . C215 C 0.0708(3) 0.1294(2) 0.83864(14) 0.0703(6) Uani 1 1 d . . . . . H215 H 0.073430 0.054549 0.865403 0.084 Uiso 1 1 calc R U . . . C216 C 0.1773(2) 0.16568(19) 0.85351(12) 0.0544(4) Uani 1 1 d . . . . . H216 H 0.249402 0.116248 0.891191 0.065 Uiso 1 1 calc R U . . . C221 C 0.27381(19) 0.40595(17) 0.91864(10) 0.0460(4) Uani 1 1 d . . . . . C222 C 0.3105(3) 0.5018(2) 0.92588(14) 0.0827(8) Uani 1 1 d . . . . . H222 H 0.352789 0.528456 0.880862 0.099 Uiso 1 1 calc R U . . . C223 C 0.2863(4) 0.5609(3) 0.99899(17) 0.0996(10) Uani 1 1 d . . . . . H223 H 0.313774 0.625537 1.002542 0.120 Uiso 1 1 calc R U . . . C224 C 0.2242(3) 0.5261(3) 1.06433(15) 0.0839(8) Uani 1 1 d . . . . . H224 H 0.206740 0.566604 1.112997 0.101 Uiso 1 1 calc R U . . . C225 C 0.1873(5) 0.4312(4) 1.0583(2) 0.1463(19) Uani 1 1 d . . . . . H225 H 0.145001 0.405459 1.103747 0.176 Uiso 1 1 calc R U . . . C226 C 0.2107(4) 0.3708(3) 0.98591(17) 0.1247(15) Uani 1 1 d . . . . . H226 H 0.183372 0.305940 0.983120 0.150 Uiso 1 1 calc R U . . . O1 O 0.60547(18) 0.4621(2) 0.75534(13) 0.0926(6) Uani 1 1 d . . . . . O2 O 0.1279(2) 0.65119(16) 0.64520(14) 0.0966(6) Uani 1 1 d . . . . . P1 P 0.43719(4) 0.27013(4) 0.62433(2) 0.03527(8) Uani 1 1 d . . . . . P2 P 0.31321(4) 0.32924(4) 0.82139(2) 0.03649(9) Uani 1 1 d . . . . . S1 S 0.32182(5) 0.07152(4) 0.60447(3) 0.04756(10) Uani 1 1 d . . . . . S2 S 0.58016(5) 0.18732(5) 0.93028(3) 0.05358(12) Uani 1 1 d . . . . . Ni Ni 0.36403(2) 0.42295(2) 0.70777(2) 0.03687(6) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0534(10) 0.0591(10) 0.0504(9) -0.0126(8) 0.0043(7) -0.0321(8) C2 0.0631(11) 0.0499(10) 0.0521(9) -0.0077(8) -0.0113(8) -0.0273(9) C3 0.0396(7) 0.0381(7) 0.0368(7) -0.0109(5) -0.0024(5) -0.0180(6) C4 0.0433(7) 0.0371(7) 0.0355(7) -0.0087(5) -0.0028(6) -0.0194(6) C5 0.0535(9) 0.0395(8) 0.0442(8) -0.0113(6) -0.0012(7) -0.0246(7) C6 0.0816(13) 0.0490(10) 0.0488(9) -0.0047(7) -0.0055(9) -0.0382(10) C7 0.1052(18) 0.0548(11) 0.0650(12) -0.0017(9) -0.0027(12) -0.0514(12) C8 0.0976(17) 0.0608(12) 0.0821(15) -0.0140(11) 0.0024(12) -0.0563(13) C9 0.0722(12) 0.0577(11) 0.0705(12) -0.0201(9) -0.0044(10) -0.0405(10) C10 0.0559(9) 0.0434(8) 0.0493(9) -0.0129(7) -0.0026(7) -0.0268(7) C11 0.0483(8) 0.0455(8) 0.0304(6) -0.0039(5) -0.0052(6) -0.0287(7) C12 0.0472(8) 0.0417(8) 0.0342(7) -0.0020(6) -0.0058(6) -0.0261(7) C13 0.0483(8) 0.0459(8) 0.0454(8) 0.0063(7) -0.0086(7) -0.0262(7) C14 0.0600(11) 0.0495(10) 0.0698(12) 0.0016(9) -0.0084(9) -0.0192(9) C15 0.0569(12) 0.0581(13) 0.1052(19) 0.0109(12) -0.0102(12) -0.0135(10) C16 0.0615(13) 0.0816(17) 0.108(2) 0.0309(15) -0.0352(13) -0.0335(13) C17 0.0667(13) 0.0847(16) 0.0717(13) 0.0171(12) -0.0303(11) -0.0446(13) C18 0.0571(10) 0.0587(10) 0.0475(9) 0.0095(7) -0.0154(7) -0.0357(9) C111 0.0399(8) 0.0728(12) 0.0361(7) -0.0121(7) 0.0028(6) -0.0240(8) C112 0.0476(11) 0.0882(17) 0.0671(13) -0.0069(12) 0.0098(9) -0.0073(11) C113 0.0491(14) 0.143(3) 0.099(2) -0.011(2) 0.0152(13) 0.0000(16) C114 0.0477(14) 0.223(5) 0.092(2) -0.041(3) 0.0195(14) -0.048(2) C115 0.0820(19) 0.192(4) 0.0763(16) -0.049(2) 0.0319(14) -0.095(2) C116 0.0653(12) 0.1070(18) 0.0603(12) -0.0265(12) 0.0192(10) -0.0554(13) C121 0.0450(8) 0.0402(8) 0.0334(7) -0.0065(6) -0.0029(6) -0.0149(6) C122 0.0532(10) 0.0738(13) 0.0380(8) -0.0101(8) 0.0000(7) -0.0153(9) C123 0.0783(14) 0.0890(16) 0.0349(9) -0.0116(9) -0.0035(9) -0.0186(12) C124 0.0800(15) 0.0715(14) 0.0499(11) -0.0142(10) -0.0262(10) -0.0048(11) C125 0.0566(12) 0.0888(17) 0.0687(14) -0.0243(12) -0.0226(10) -0.0007(11) C126 0.0465(9) 0.0746(13) 0.0506(10) -0.0210(9) -0.0047(7) -0.0090(9) C211 0.0448(8) 0.0550(9) 0.0364(7) -0.0169(6) 0.0088(6) -0.0299(7) C212 0.0469(9) 0.0650(11) 0.0520(9) -0.0087(8) 0.0024(7) -0.0282(8) C213 0.0508(10) 0.1026(18) 0.0623(12) -0.0167(12) 0.0008(9) -0.0415(12) C214 0.0679(13) 0.1113(19) 0.0653(12) -0.0292(12) 0.0117(10) -0.0649(14) C215 0.0885(15) 0.0880(16) 0.0673(13) -0.0150(11) 0.0145(11) -0.0684(14) C216 0.0643(11) 0.0665(12) 0.0495(9) -0.0076(8) 0.0045(8) -0.0439(10) C221 0.0584(10) 0.0535(9) 0.0366(7) -0.0169(7) 0.0073(7) -0.0313(8) C222 0.149(2) 0.0815(15) 0.0578(12) -0.0355(11) 0.0380(14) -0.0839(17) C223 0.176(3) 0.0993(19) 0.0725(15) -0.0515(14) 0.0377(17) -0.098(2) C224 0.116(2) 0.0966(18) 0.0548(12) -0.0449(12) 0.0196(13) -0.0530(16) C225 0.259(5) 0.194(4) 0.0804(19) -0.089(2) 0.099(3) -0.176(4) C226 0.225(4) 0.164(3) 0.0756(16) -0.0757(19) 0.084(2) -0.161(3) O1 0.0694(10) 0.1339(16) 0.1049(14) -0.0320(12) -0.0003(9) -0.0676(11) O2 0.0885(12) 0.0620(10) 0.1234(16) 0.0011(10) -0.0497(11) -0.0149(9) P1 0.03758(18) 0.04108(19) 0.03014(16) -0.00693(14) 0.00113(13) -0.01866(15) P2 0.0453(2) 0.0425(2) 0.03079(16) -0.01026(14) 0.00356(14) -0.02590(17) S1 0.0569(2) 0.0501(2) 0.0430(2) -0.01024(17) -0.01142(17) -0.02745(19) S2 0.0694(3) 0.0662(3) 0.0396(2) -0.00599(18) -0.01487(18) -0.0413(2) Ni 0.04465(11) 0.03901(11) 0.03385(10) -0.00683(7) 0.00163(7) -0.02358(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.130(2) . ? C1 Ni 1.7770(18) . ? C2 O2 1.139(2) . ? C2 Ni 1.766(2) . ? C3 C4 1.365(2) . ? C3 S1 1.7441(15) . ? C3 P1 1.8259(16) . ? C4 C5 1.440(2) . ? C4 C12 1.480(2) . ? C5 C6 1.398(3) . ? C5 C10 1.404(2) . ? C6 C7 1.375(3) . ? C7 C8 1.387(3) . ? C8 C9 1.368(3) . ? C9 C10 1.401(2) . ? C10 S1 1.7308(19) . ? C11 C12 1.367(2) . ? C11 S2 1.7394(15) . ? C11 P2 1.8181(19) . ? C12 C13 1.441(2) . ? C13 C18 1.399(2) . ? C13 C14 1.401(3) . ? C14 C15 1.381(3) . ? C15 C16 1.382(4) . ? C16 C17 1.368(4) . ? C17 C18 1.398(3) . ? C18 S2 1.731(2) . ? C111 C112 1.376(3) . ? C111 C116 1.394(3) . ? C111 P1 1.8278(18) . ? C112 C113 1.392(4) . ? C113 C114 1.353(6) . ? C114 C115 1.360(6) . ? C115 C116 1.396(3) . ? C121 C122 1.380(2) . ? C121 C126 1.386(2) . ? C121 P1 1.8298(16) . ? C122 C123 1.392(3) . ? C123 C124 1.362(3) . ? C124 C125 1.381(3) . ? C125 C126 1.382(3) . ? C211 C216 1.385(3) . ? C211 C212 1.388(3) . ? C211 P2 1.8257(16) . ? C212 C213 1.387(3) . ? C213 C214 1.369(4) . ? C214 C215 1.368(4) . ? C215 C216 1.394(3) . ? C221 C222 1.357(3) . ? C221 C226 1.365(3) . ? C221 P2 1.8314(16) . ? C222 C223 1.387(3) . ? C223 C224 1.335(4) . ? C224 C225 1.344(4) . ? C225 C226 1.385(3) . ? P1 Ni 2.2162(9) . ? P2 Ni 2.1963(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Ni 178.56(19) . . ? O2 C2 Ni 175.94(18) . . ? C4 C3 S1 111.91(11) . . ? C4 C3 P1 127.02(11) . . ? S1 C3 P1 120.96(9) . . ? C3 C4 C5 113.07(13) . . ? C3 C4 C12 126.34(14) . . ? C5 C4 C12 120.47(14) . . ? C6 C5 C10 119.50(15) . . ? C6 C5 C4 128.66(15) . . ? C10 C5 C4 111.73(15) . . ? C7 C6 C5 119.02(18) . . ? C6 C7 C8 120.9(2) . . ? C9 C8 C7 121.68(18) . . ? C8 C9 C10 118.08(18) . . ? C9 C10 C5 120.83(18) . . ? C9 C10 S1 127.75(15) . . ? C5 C10 S1 111.40(12) . . ? C12 C11 S2 111.95(12) . . ? C12 C11 P2 126.61(11) . . ? S2 C11 P2 120.09(9) . . ? C11 C12 C13 112.98(14) . . ? C11 C12 C4 123.26(14) . . ? C13 C12 C4 123.63(14) . . ? C18 C13 C14 118.94(17) . . ? C18 C13 C12 111.67(16) . . ? C14 C13 C12 129.34(16) . . ? C15 C14 C13 118.9(2) . . ? C14 C15 C16 121.5(2) . . ? C17 C16 C15 120.8(2) . . ? C16 C17 C18 118.6(2) . . ? C17 C18 C13 121.3(2) . . ? C17 C18 S2 127.10(17) . . ? C13 C18 S2 111.60(13) . . ? C112 C111 C116 119.16(19) . . ? C112 C111 P1 123.74(17) . . ? C116 C111 P1 117.08(16) . . ? C111 C112 C113 119.8(3) . . ? C114 C113 C112 120.8(3) . . ? C113 C114 C115 120.3(3) . . ? C114 C115 C116 120.4(3) . . ? C111 C116 C115 119.5(3) . . ? C122 C121 C126 118.57(16) . . ? C122 C121 P1 123.60(13) . . ? C126 C121 P1 117.77(13) . . ? C121 C122 C123 120.73(19) . . ? C124 C123 C122 120.16(19) . . ? C123 C124 C125 119.75(18) . . ? C124 C125 C126 120.3(2) . . ? C125 C126 C121 120.46(19) . . ? C216 C211 C212 118.66(16) . . ? C216 C211 P2 124.41(14) . . ? C212 C211 P2 116.89(13) . . ? C213 C212 C211 120.8(2) . . ? C214 C213 C212 119.9(2) . . ? C215 C214 C213 120.11(19) . . ? C214 C215 C216 120.5(2) . . ? C211 C216 C215 120.0(2) . . ? C222 C221 C226 117.33(18) . . ? C222 C221 P2 119.12(14) . . ? C226 C221 P2 123.54(15) . . ? C221 C222 C223 121.4(2) . . ? C224 C223 C222 120.8(2) . . ? C223 C224 C225 118.6(2) . . ? C224 C225 C226 121.5(3) . . ? C221 C226 C225 120.4(2) . . ? C3 P1 C111 103.34(9) . . ? C3 P1 C121 100.24(7) . . ? C111 P1 C121 103.24(8) . . ? C3 P1 Ni 116.25(5) . . ? C111 P1 Ni 114.68(7) . . ? C121 P1 Ni 116.97(6) . . ? C11 P2 C211 105.37(8) . . ? C11 P2 C221 102.00(8) . . ? C211 P2 C221 104.40(8) . . ? C11 P2 Ni 106.46(6) . . ? C211 P2 Ni 117.31(6) . . ? C221 P2 Ni 119.44(6) . . ? C10 S1 C3 91.82(8) . . ? C18 S2 C11 91.79(9) . . ? C2 Ni C1 114.72(9) . . ? C2 Ni P2 112.87(7) . . ? C1 Ni P2 105.44(7) . . ? C2 Ni P1 114.26(6) . . ? C1 Ni P1 107.44(7) . . ? P2 Ni P1 100.85(3) . . ? _refine_diff_density_max 0.421 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.052 _shelx_res_file ; TITL nice in P-1 shelx.res created by SHELXL-2017/1 at 14:55:08 on 05-Mar-2019 CELL 0.71073 10.5390 11.8108 15.9940 83.931 88.181 65.243 ZERR 2.00 0.0021 0.0024 0.0032 0.030 0.030 0.030 LATT 1 SFAC C H O P S NI UNIT 84 56 4 4 4 2 MERG 2 FMAP 2 PLAN 25 ACTA L.S. 1 WGHT 0.056700 0.319000 FVAR 0.29238 C1 1 0.511912 0.447220 0.735794 11.00000 0.05342 0.05909 = 0.05042 -0.01259 0.00430 -0.03208 C2 1 0.220265 0.559828 0.667174 11.00000 0.06307 0.04990 = 0.05210 -0.00765 -0.01129 -0.02729 C3 1 0.414931 0.128585 0.663080 11.00000 0.03957 0.03814 = 0.03677 -0.01087 -0.00238 -0.01798 C4 1 0.457573 0.059994 0.739205 11.00000 0.04326 0.03714 = 0.03552 -0.00871 -0.00284 -0.01941 C5 1 0.415939 -0.042117 0.752341 11.00000 0.05352 0.03949 = 0.04424 -0.01130 -0.00120 -0.02462 C6 1 0.437795 -0.128525 0.823179 11.00000 0.08155 0.04905 = 0.04876 -0.00466 -0.00549 -0.03816 AFIX 43 H6 2 0.490456 -0.128279 0.868673 11.00000 -1.20000 AFIX 0 C7 1 0.380310 -0.213880 0.824616 11.00000 0.10519 0.05482 = 0.06502 -0.00168 -0.00271 -0.05139 AFIX 43 H7 2 0.395492 -0.272487 0.871167 11.00000 -1.20000 AFIX 0 C8 1 0.299985 -0.213743 0.757570 11.00000 0.09762 0.06084 = 0.08208 -0.01400 0.00241 -0.05627 AFIX 43 H8 2 0.260320 -0.271104 0.760720 11.00000 -1.20000 AFIX 0 C9 1 0.277592 -0.131369 0.686897 11.00000 0.07222 0.05773 = 0.07047 -0.02010 -0.00442 -0.04048 AFIX 43 H9 2 0.224673 -0.132916 0.641952 11.00000 -1.20000 AFIX 0 C10 1 0.336677 -0.044644 0.684197 11.00000 0.05593 0.04338 = 0.04933 -0.01290 -0.00260 -0.02675 C11 1 0.470269 0.188522 0.850989 11.00000 0.04834 0.04548 = 0.03040 -0.00387 -0.00519 -0.02874 C12 1 0.531051 0.086587 0.806652 11.00000 0.04717 0.04168 = 0.03420 -0.00202 -0.00580 -0.02610 C13 1 0.670166 0.003722 0.836315 11.00000 0.04826 0.04587 = 0.04542 0.00628 -0.00860 -0.02623 C14 1 0.765185 -0.107092 0.805672 11.00000 0.05997 0.04949 = 0.06976 0.00164 -0.00836 -0.01916 AFIX 43 H14 2 0.740914 -0.138056 0.760589 11.00000 -1.20000 AFIX 0 C15 1 0.895482 -0.169557 0.843541 11.00000 0.05691 0.05806 = 0.10521 0.01092 -0.01020 -0.01351 AFIX 43 H15 2 0.958906 -0.243295 0.823578 11.00000 -1.20000 AFIX 0 C16 1 0.933739 -0.124950 0.910437 11.00000 0.06155 0.08164 = 0.10797 0.03085 -0.03519 -0.03346 AFIX 43 H16 2 1.022090 -0.169192 0.934846 11.00000 -1.20000 AFIX 0 C17 1 0.843327 -0.016553 0.941219 11.00000 0.06674 0.08471 = 0.07166 0.01705 -0.03026 -0.04458 AFIX 43 H17 2 0.869212 0.013250 0.986305 11.00000 -1.20000 AFIX 0 C18 1 0.711157 0.048460 0.903428 11.00000 0.05708 0.05871 = 0.04752 0.00950 -0.01543 -0.03566 C111 1 0.622760 0.210749 0.599067 11.00000 0.03989 0.07279 = 0.03609 -0.01206 0.00284 -0.02404 C112 1 0.711661 0.085391 0.604690 11.00000 0.04756 0.08824 = 0.06713 -0.00688 0.00976 -0.00730 AFIX 43 H112 2 0.677210 0.025254 0.618972 11.00000 -1.20000 AFIX 0 C113 1 0.853340 0.048833 0.588937 11.00000 0.04913 0.14350 = 0.09870 -0.01089 0.01515 -0.00005 AFIX 43 H113 2 0.913623 -0.035875 0.594535 11.00000 -1.20000 AFIX 0 C114 1 0.904403 0.134986 0.565590 11.00000 0.04766 0.22329 = 0.09207 -0.04103 0.01945 -0.04790 AFIX 43 H114 2 0.999171 0.109125 0.554871 11.00000 -1.20000 AFIX 0 C115 1 0.817771 0.259232 0.557727 11.00000 0.08201 0.19239 = 0.07632 -0.04937 0.03195 -0.09463 AFIX 43 H115 2 0.853378 0.317870 0.540872 11.00000 -1.20000 AFIX 0 C116 1 0.675721 0.299263 0.574807 11.00000 0.06526 0.10699 = 0.06032 -0.02654 0.01919 -0.05538 AFIX 43 H116 2 0.616839 0.384327 0.570044 11.00000 -1.20000 AFIX 0 C121 1 0.351805 0.304783 0.521064 11.00000 0.04497 0.04016 = 0.03341 -0.00650 -0.00292 -0.01492 C122 1 0.423588 0.276588 0.446931 11.00000 0.05324 0.07385 = 0.03804 -0.01010 0.00005 -0.01531 AFIX 43 H122 2 0.520767 0.240878 0.447897 11.00000 -1.20000 AFIX 0 C123 1 0.352159 0.301004 0.370742 11.00000 0.07830 0.08896 = 0.03493 -0.01156 -0.00348 -0.01855 AFIX 43 H123 2 0.401690 0.282941 0.321090 11.00000 -1.20000 AFIX 0 C124 1 0.209840 0.351305 0.368719 11.00000 0.07999 0.07147 = 0.04988 -0.01419 -0.02618 -0.00478 AFIX 43 H124 2 0.162179 0.367168 0.317824 11.00000 -1.20000 AFIX 0 C125 1 0.136648 0.378639 0.442499 11.00000 0.05657 0.08883 = 0.06873 -0.02430 -0.02260 -0.00068 AFIX 43 H125 2 0.039561 0.411594 0.441341 11.00000 -1.20000 AFIX 0 C126 1 0.207007 0.357249 0.518075 11.00000 0.04647 0.07464 = 0.05060 -0.02103 -0.00465 -0.00898 AFIX 43 H126 2 0.156851 0.378204 0.567267 11.00000 -1.20000 AFIX 0 C211 1 0.175655 0.275408 0.812150 11.00000 0.04477 0.05500 = 0.03636 -0.01689 0.00882 -0.02986 C212 1 0.065201 0.348410 0.757550 11.00000 0.04691 0.06502 = 0.05203 -0.00870 0.00237 -0.02820 AFIX 43 H212 2 0.063015 0.422077 0.729088 11.00000 -1.20000 AFIX 0 C213 1 -0.041947 0.312807 0.744932 11.00000 0.05081 0.10263 = 0.06231 -0.01674 0.00081 -0.04154 AFIX 43 H213 2 -0.116641 0.363537 0.709288 11.00000 -1.20000 AFIX 0 C214 1 -0.037685 0.202941 0.784979 11.00000 0.06794 0.11130 = 0.06534 -0.02924 0.01169 -0.06492 AFIX 43 H214 2 -0.108644 0.178275 0.775688 11.00000 -1.20000 AFIX 0 C215 1 0.070752 0.129372 0.838637 11.00000 0.08850 0.08804 = 0.06726 -0.01499 0.01453 -0.06836 AFIX 43 H215 2 0.073430 0.054549 0.865403 11.00000 -1.20000 AFIX 0 C216 1 0.177270 0.165677 0.853511 11.00000 0.06431 0.06648 = 0.04951 -0.00761 0.00453 -0.04393 AFIX 43 H216 2 0.249402 0.116248 0.891191 11.00000 -1.20000 AFIX 0 C221 1 0.273810 0.405946 0.918638 11.00000 0.05843 0.05352 = 0.03656 -0.01693 0.00729 -0.03126 C222 1 0.310524 0.501818 0.925879 11.00000 0.14941 0.08152 = 0.05778 -0.03545 0.03801 -0.08391 AFIX 43 H222 2 0.352789 0.528456 0.880862 11.00000 -1.20000 AFIX 0 C223 1 0.286339 0.560890 0.998995 11.00000 0.17588 0.09934 = 0.07248 -0.05151 0.03767 -0.09800 AFIX 43 H223 2 0.313774 0.625537 1.002542 11.00000 -1.20000 AFIX 0 C224 1 0.224161 0.526069 1.064330 11.00000 0.11648 0.09665 = 0.05479 -0.04488 0.01962 -0.05302 AFIX 43 H224 2 0.206740 0.566604 1.112997 11.00000 -1.20000 AFIX 0 C225 1 0.187252 0.431159 1.058294 11.00000 0.25854 0.19430 = 0.08041 -0.08892 0.09944 -0.17634 AFIX 43 H225 2 0.145001 0.405459 1.103747 11.00000 -1.20000 AFIX 0 C226 1 0.210736 0.370793 0.985906 11.00000 0.22459 0.16417 = 0.07557 -0.07572 0.08414 -0.16072 AFIX 43 H226 2 0.183372 0.305940 0.983120 11.00000 -1.20000 AFIX 0 O1 3 0.605466 0.462147 0.755341 11.00000 0.06943 0.13388 = 0.10493 -0.03196 -0.00033 -0.06760 O2 3 0.127881 0.651192 0.645195 11.00000 0.08853 0.06199 = 0.12343 0.00113 -0.04970 -0.01489 P1 4 0.437191 0.270128 0.624328 11.00000 0.03758 0.04108 = 0.03014 -0.00693 0.00113 -0.01866 P2 4 0.313210 0.329245 0.821393 11.00000 0.04528 0.04245 = 0.03079 -0.01026 0.00356 -0.02590 S1 5 0.321822 0.071517 0.604470 11.00000 0.05692 0.05007 = 0.04303 -0.01024 -0.01142 -0.02745 S2 5 0.580161 0.187323 0.930284 11.00000 0.06942 0.06617 = 0.03965 -0.00599 -0.01487 -0.04132 NI 6 0.364028 0.422950 0.707767 11.00000 0.04465 0.03901 = 0.03385 -0.00683 0.00163 -0.02358 HKLF 4 REM nice in P-1 REM R1 = 0.0360 for 8977 Fo > 4sig(Fo) and 0.0529 for all 11837 data REM 442 parameters refined using 0 restraints END WGHT 0.0564 0.3246 REM Highest difference peak 0.421, deepest hole -0.365, 1-sigma level 0.052 Q1 1 0.1630 0.4411 0.9557 11.00000 0.05 0.42 Q2 1 0.2456 0.4827 0.9062 11.00000 0.05 0.38 Q3 1 0.3989 0.3535 0.7222 11.00000 0.05 0.38 Q4 1 0.3823 0.2601 0.8435 11.00000 0.05 0.37 Q5 1 0.3207 0.4274 0.6712 11.00000 0.05 0.37 Q6 1 0.2593 0.3414 0.9901 11.00000 0.05 0.34 Q7 1 0.6201 0.1172 0.9372 11.00000 0.05 0.33 Q8 1 0.2834 0.4956 0.6899 11.00000 0.05 0.33 Q9 1 0.4994 0.0743 0.7705 11.00000 0.05 0.33 Q10 1 0.4195 0.4168 0.7444 11.00000 0.05 0.32 Q11 1 0.1410 0.5181 1.0282 11.00000 0.05 0.32 Q12 1 0.2959 0.3546 0.8831 11.00000 0.05 0.32 Q13 1 0.3921 0.2795 0.5750 11.00000 0.05 0.30 Q14 1 0.3808 0.3484 0.6645 11.00000 0.05 0.30 Q15 1 0.1633 0.4472 0.4195 11.00000 0.05 0.29 Q16 1 0.4181 0.2010 0.6495 11.00000 0.05 0.29 Q17 1 0.3274 0.3822 0.7623 11.00000 0.05 0.28 Q18 1 0.4183 0.4699 0.9005 11.00000 0.05 0.28 Q19 1 0.2491 0.3988 1.0645 11.00000 0.05 0.28 Q20 1 0.2185 0.4228 0.4965 11.00000 0.05 0.27 Q21 1 0.3773 -0.0439 0.7217 11.00000 0.05 0.27 Q22 1 0.2796 0.1164 0.5641 11.00000 0.05 0.27 Q23 1 0.3574 0.4407 0.9487 11.00000 0.05 0.26 Q24 1 0.5014 0.1487 0.8191 11.00000 0.05 0.26 Q25 1 0.5999 0.0391 0.8173 11.00000 0.05 0.26 ; _shelx_res_checksum 85307 _shelx_hkl_file ; 0 -4 -23 1.89 0.57 0 -3 -23 0.74 0.51 1 -3 -23 1.34 0.53 0 -2 -23 3.75 0.65 -2 -8 -22 1.18 0.54 -1 -8 -22 0.42 0.43 -3 -7 -22 3.32 0.59 -2 -7 -22 1.64 0.51 -1 -7 -22 3.86 0.54 0 -7 -22 7.18 0.83 -4 -6 -22 1.38 0.57 -3 -6 -22 0.34 0.48 -2 -6 -22 0.49 0.48 -1 -6 -22 0.34 0.44 0 -6 -22 0.56 0.45 1 -6 -22 1.16 0.47 -4 -5 -22 16.21 1.04 -3 -5 -22 0.37 0.48 -2 -5 -22 10.55 1.03 -1 -5 -22 12.15 0.90 0 -5 -22 1.89 0.50 1 -5 -22 4.20 0.58 2 -5 -22 10.80 0.90 -4 -4 -22 5.21 0.66 -3 -4 -22 1.38 0.56 -2 -4 -22 3.33 0.58 -1 -4 -22 0.60 0.48 0 -4 -22 0.51 0.47 1 -4 -22 1.77 0.49 2 -4 -22 0.20 0.45 3 -4 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0.78 -3 -7 0 62.91 0.49 -2 -7 0 8.89 0.25 -1 -7 0 1.11 0.13 0 -7 0 22.78 0.29 1 -7 0 67.80 0.38 2 -7 0 22.80 0.42 3 -7 0 4.39 0.34 4 -7 0 -0.05 0.20 5 -7 0 4.07 0.30 6 -7 0 4.24 0.33 7 -7 0 -0.12 0.27 8 -7 0 0.38 0.30 9 -7 0 -0.13 0.47 10 -7 0 2.77 0.61 -15 -6 0 3.12 0.63 -14 -6 0 0.91 0.35 -13 -6 0 1.00 0.32 -12 -6 0 23.64 0.85 -11 -6 0 92.28 1.27 -10 -6 0 38.00 0.85 -9 -6 0 1.85 0.33 -8 -6 0 3.62 0.37 -7 -6 0 9.36 0.48 -6 -6 0 1.54 0.13 -5 -6 0 60.48 0.41 -4 -6 0 1.93 0.15 -3 -6 0 91.64 0.52 -2 -6 0 109.85 0.57 -1 -6 0 304.48 1.03 0 -6 0 32.07 0.30 1 -6 0 30.11 0.23 2 -6 0 61.17 0.56 3 -6 0 118.75 0.80 4 -6 0 8.46 0.36 5 -6 0 1.03 0.21 6 -6 0 1.75 0.25 7 -6 0 3.51 0.31 8 -6 0 6.72 0.50 9 -6 0 -0.16 0.45 10 -6 0 0.75 0.54 -15 -5 0 -0.54 0.57 -14 -5 0 -0.28 0.49 -13 -5 0 0.75 0.31 -12 -5 0 41.29 0.69 -11 -5 0 40.94 0.94 -10 -5 0 3.04 0.38 -9 -5 0 91.97 1.12 -8 -5 0 135.02 1.24 -7 -5 0 10.23 0.47 -6 -5 0 6.82 0.38 -5 -5 0 206.95 0.67 -4 -5 0 47.87 0.34 -3 -5 0 189.92 0.66 -2 -5 0 106.67 0.51 -1 -5 0 54.68 0.36 0 -5 0 0.31 0.08 1 -5 0 26.68 0.20 2 -5 0 38.58 0.42 3 -5 0 51.65 0.52 4 -5 0 63.20 0.60 5 -5 0 6.32 0.35 6 -5 0 -0.11 0.19 7 -5 0 5.59 0.40 8 -5 0 11.03 0.49 9 -5 0 0.06 0.42 10 -5 0 -0.27 0.46 11 -5 0 -0.11 0.49 -14 -4 0 0.37 0.53 -13 -4 0 6.03 0.45 -12 -4 0 15.52 0.55 -11 -4 0 1.26 0.26 -10 -4 0 75.16 1.03 -9 -4 0 116.75 1.19 -8 -4 0 28.18 0.64 -7 -4 0 2.15 0.27 -6 -4 0 75.70 0.80 -5 -4 0 12.87 0.38 -4 -4 0 0.46 0.07 -3 -4 0 3.49 0.14 -2 -4 0 297.86 1.69 -1 -4 0 493.95 2.12 0 -4 0 115.46 0.43 1 -4 0 11.08 0.12 2 -4 0 8.10 0.23 3 -4 0 3.22 0.21 4 -4 0 6.26 0.28 5 -4 0 74.89 0.65 6 -4 0 6.56 0.34 7 -4 0 36.27 0.57 8 -4 0 1.77 0.26 9 -4 0 9.77 0.81 10 -4 0 3.50 0.55 11 -4 0 -0.18 0.50 -14 -3 0 0.00 0.54 -13 -3 0 1.49 0.53 -12 -3 0 -0.29 0.26 -11 -3 0 6.05 0.42 -10 -3 0 0.34 0.22 -9 -3 0 0.19 0.27 -8 -3 0 7.66 0.46 -7 -3 0 2.20 0.25 -6 -3 0 2.37 0.23 -5 -3 0 30.80 0.49 -4 -3 0 371.50 2.88 -3 -3 0 3.84 0.11 -2 -3 0 180.79 1.27 -1 -3 0 53.52 0.29 0 -3 0 11.78 0.15 1 -3 0 330.76 1.75 2 -3 0 284.26 1.71 3 -3 0 29.64 0.34 4 -3 0 48.90 0.46 5 -3 0 165.37 0.85 6 -3 0 226.29 1.06 7 -3 0 -0.10 0.17 8 -3 0 25.35 0.50 9 -3 0 18.08 0.82 10 -3 0 3.54 0.53 11 -3 0 0.14 0.49 12 -3 0 -0.44 0.51 -14 -2 0 1.27 0.62 -13 -2 0 1.77 0.56 -12 -2 0 2.74 0.51 -11 -2 0 -0.22 0.22 -10 -2 0 5.77 0.38 -9 -2 0 0.01 0.19 -8 -2 0 72.80 0.62 -7 -2 0 54.82 0.69 -6 -2 0 105.78 0.85 -5 -2 0 186.89 1.01 -4 -2 0 1.32 0.15 -3 -2 0 154.12 0.94 -2 -2 0 1853.84 16.98 -1 -2 0 624.34 2.69 0 -2 0 1.26 0.13 1 -2 0 740.39 3.78 2 -2 0 36.00 0.29 3 -2 0 2.37 0.16 4 -2 0 0.47 0.11 5 -2 0 0.26 0.12 6 -2 0 7.41 0.28 7 -2 0 17.53 0.38 8 -2 0 20.11 0.41 9 -2 0 4.18 0.45 10 -2 0 1.41 0.43 11 -2 0 -0.09 0.44 12 -2 0 2.48 0.56 -14 -1 0 3.00 0.68 -13 -1 0 2.84 0.62 -12 -1 0 1.55 0.52 -11 -1 0 -0.13 0.40 -10 -1 0 0.10 0.21 -9 -1 0 6.46 0.34 -8 -1 0 3.58 0.26 -7 -1 0 16.36 0.42 -6 -1 0 15.37 0.28 -5 -1 0 50.97 0.53 -4 -1 0 47.54 0.46 -3 -1 0 21.22 0.31 -2 -1 0 244.69 1.65 -1 -1 0 370.34 1.79 0 -1 0 0.84 0.05 1 -1 0 254.55 1.18 2 -1 0 101.86 0.50 3 -1 0 2.28 0.14 4 -1 0 19.98 0.26 5 -1 0 127.90 0.62 6 -1 0 2.27 0.16 7 -1 0 143.38 0.77 8 -1 0 98.96 0.70 9 -1 0 0.33 0.32 10 -1 0 2.20 0.42 11 -1 0 12.42 0.83 12 -1 0 6.00 0.65 13 -1 0 0.17 0.55 -13 0 0 -0.30 0.54 -12 0 0 -0.42 0.51 -11 0 0 -0.03 0.44 -10 0 0 3.76 0.47 -9 0 0 5.51 0.33 -8 0 0 33.80 0.46 -7 0 0 0.09 0.15 -6 0 0 7.67 0.23 -5 0 0 0.79 0.12 -4 0 0 422.30 2.47 -3 0 0 283.56 1.66 -2 0 0 401.16 1.78 -1 0 0 1411.13 9.67 1 0 0 1419.50 7.13 2 0 0 402.43 1.46 3 0 0 272.98 1.13 4 0 0 405.80 1.78 5 0 0 0.87 0.10 6 0 0 7.71 0.25 7 0 0 -0.05 0.12 8 0 0 34.93 0.45 9 0 0 5.79 0.56 10 0 0 2.89 0.40 11 0 0 0.10 0.40 12 0 0 0.33 0.45 13 0 0 0.30 0.53 -13 1 0 0.03 0.61 -12 1 0 5.95 0.68 -11 1 0 10.64 0.83 -10 1 0 2.33 0.47 -9 1 0 0.42 0.35 -8 1 0 95.39 0.70 -7 1 0 140.40 0.73 -6 1 0 2.19 0.19 -5 1 0 128.60 0.75 -4 1 0 20.21 0.23 -3 1 0 2.95 0.13 -2 1 0 104.26 0.72 -1 1 0 251.31 1.57 0 1 0 1.27 0.04 1 1 0 367.60 1.60 2 1 0 251.54 1.54 3 1 0 20.91 0.13 4 1 0 48.57 0.25 5 1 0 50.60 0.27 6 1 0 15.70 0.21 7 1 0 16.63 0.25 9 1 0 7.15 0.52 10 1 0 0.60 0.34 11 1 0 -0.54 0.35 12 1 0 1.52 0.46 13 1 0 2.78 0.56 14 1 0 2.95 0.63 -12 2 0 1.85 0.62 -11 2 0 -0.85 0.48 -10 2 0 0.97 0.47 -9 2 0 5.24 0.52 -8 2 0 19.95 0.73 -7 2 0 17.71 0.66 -6 2 0 7.94 0.24 -5 2 0 0.18 0.11 -4 2 0 0.36 0.09 -3 2 0 2.44 0.11 -2 2 0 37.69 0.45 -1 2 0 732.58 12.44 0 2 0 1.25 0.15 1 2 0 623.25 2.90 2 2 0 1826.54 11.93 3 2 0 150.68 0.51 4 2 0 1.36 0.12 5 2 0 185.93 0.87 6 2 0 105.95 0.65 7 2 0 56.72 0.55 8 2 0 72.92 0.95 9 2 0 0.06 0.26 10 2 0 5.97 0.56 11 2 0 -0.14 0.34 12 2 0 2.47 0.50 13 2 0 2.04 0.53 14 2 0 1.81 0.55 -12 3 0 -0.11 0.60 -11 3 0 -0.15 0.54 -10 3 0 3.80 0.57 -9 3 0 18.51 0.85 -8 3 0 25.07 0.82 -7 3 0 -0.14 0.34 -6 3 0 219.29 1.60 -5 3 0 162.97 0.53 -4 3 0 48.43 0.68 -3 3 0 28.73 0.51 -2 3 0 286.50 1.51 -1 3 0 334.13 2.55 0 3 0 11.86 0.30 1 3 0 54.21 0.29 2 3 0 171.04 0.69 3 3 0 3.69 0.14 4 3 0 357.70 1.82 5 3 0 30.09 0.33 6 3 0 1.89 0.15 7 3 0 2.54 0.22 8 3 0 7.29 0.33 9 3 0 0.01 0.27 10 3 0 0.57 0.30 11 3 0 6.35 0.63 12 3 0 0.01 0.40 13 3 0 1.55 0.51 14 3 0 0.33 0.51 -11 4 0 -0.61 0.59 -10 4 0 3.77 0.64 -9 4 0 10.68 0.82 -8 4 0 2.64 0.48 -7 4 0 35.95 0.88 -6 4 0 6.09 0.58 -4 4 0 6.77 0.45 -3 4 0 3.52 0.36 -2 4 0 8.22 0.37 -1 4 0 11.29 0.36 0 4 0 114.44 0.51 1 4 0 490.63 2.12 2 4 0 296.47 1.41 3 4 0 3.19 0.14 4 4 0 0.37 0.10 5 4 0 12.39 0.24 6 4 0 74.42 0.54 7 4 0 2.75 0.22 8 4 0 28.00 0.46 9 4 0 113.23 0.85 10 4 0 75.85 0.79 11 4 0 1.27 0.37 12 4 0 15.73 0.78 13 4 0 7.74 0.78 14 4 0 -0.14 0.50 -11 5 0 -0.18 0.62 -10 5 0 -0.07 0.57 -9 5 0 0.06 0.51 -8 5 0 10.45 0.80 -7 5 0 6.10 0.68 -6 5 0 -0.09 0.37 -5 5 0 5.88 0.57 -4 5 0 62.98 0.95 -3 5 0 50.63 0.77 -2 5 0 37.61 0.63 -1 5 0 26.20 0.52 0 5 0 0.24 0.11 1 5 0 55.20 0.38 2 5 0 106.58 0.50 3 5 0 187.39 0.68 4 5 0 46.86 0.37 5 5 0 204.95 0.79 6 5 0 7.78 0.25 7 5 0 10.61 0.30 8 5 0 130.60 0.83 9 5 0 90.25 0.77 10 5 0 3.15 0.28 11 5 0 39.58 0.67 12 5 0 42.00 1.02 13 5 0 1.13 0.45 14 5 0 -0.16 0.44 15 5 0 0.27 0.50 -10 6 0 -0.03 0.62 -9 6 0 -0.67 0.54 -8 6 0 4.84 0.63 -7 6 0 3.89 0.55 -6 6 0 2.12 0.45 -5 6 0 1.53 0.40 -4 6 0 8.31 0.59 -3 6 0 114.66 1.18 -2 6 0 61.42 0.85 -1 6 0 30.97 0.61 0 6 0 31.50 0.37 1 6 0 307.79 1.15 2 6 0 109.87 0.57 3 6 0 89.98 0.51 4 6 0 2.04 0.18 5 6 0 58.22 0.46 6 6 0 1.86 0.16 7 6 0 9.59 0.30 8 6 0 3.87 0.29 9 6 0 1.81 0.23 10 6 0 36.98 0.58 11 6 0 90.24 0.89 12 6 0 23.62 0.62 13 6 0 1.73 0.46 14 6 0 1.82 0.50 15 6 0 3.23 0.57 -9 7 0 -0.02 0.60 -8 7 0 0.31 0.56 -7 7 0 -0.03 0.48 -6 7 0 4.13 0.55 -5 7 0 3.73 0.49 -4 7 0 0.36 0.39 -3 7 0 6.29 0.57 -2 7 0 22.53 0.67 -1 7 0 67.95 0.59 0 7 0 23.45 0.37 1 7 0 1.15 0.15 2 7 0 8.71 0.24 3 7 0 62.47 0.48 4 7 0 170.63 0.77 5 7 0 210.05 1.27 6 7 0 13.05 0.32 7 7 0 137.45 0.81 8 7 0 77.21 0.67 9 7 0 4.49 0.32 10 7 0 4.43 0.37 11 7 0 13.04 0.47 12 7 0 4.45 0.36 13 7 0 13.25 0.57 14 7 0 2.68 0.51 15 7 0 1.84 0.52 -9 8 0 0.59 0.69 -8 8 0 0.49 0.63 -7 8 0 -0.36 0.56 -6 8 0 4.82 0.62 -5 8 0 0.44 0.46 -4 8 0 0.31 0.40 -3 8 0 -0.05 0.35 -2 8 0 1.93 0.39 -1 8 0 106.57 0.78 0 8 0 116.43 0.76 1 8 0 23.73 0.39 2 8 0 30.08 0.41 3 8 0 438.72 1.58 4 8 0 178.32 0.84 5 8 0 9.52 0.30 6 8 0 132.87 0.78 7 8 0 54.38 0.56 8 8 0 6.85 0.33 9 8 0 45.18 0.59 10 8 0 25.88 0.53 11 8 0 0.64 0.25 12 8 0 5.92 0.48 13 8 0 4.65 0.38 14 8 0 -0.13 0.32 15 8 0 0.45 0.48 -8 9 0 2.28 0.72 -7 9 0 2.71 0.69 -6 9 0 -0.49 0.52 -5 9 0 11.34 0.87 -4 9 0 10.60 0.84 -3 9 0 8.99 0.71 -2 9 0 5.39 0.36 -1 9 0 9.99 0.37 0 9 0 1.48 0.22 1 9 0 54.17 0.57 2 9 0 137.05 0.82 3 9 0 15.33 0.37 4 9 0 42.88 0.49 5 9 0 171.42 0.90 6 9 0 22.20 0.41 7 9 0 46.70 0.55 8 9 0 0.73 0.21 9 9 0 4.62 0.35 10 9 0 5.05 0.39 11 9 0 0.55 0.26 12 9 0 -0.11 0.25 13 9 0 2.35 0.33 14 9 0 1.23 0.35 15 9 0 0.03 0.45 -7 10 0 0.11 0.65 -6 10 0 3.47 0.68 -5 10 0 2.61 0.62 -4 10 0 2.86 0.56 -3 10 0 1.60 0.28 -2 10 0 6.03 0.43 -1 10 0 -0.02 0.21 0 10 0 0.31 0.21 1 10 0 8.79 0.36 2 10 0 16.83 0.40 3 10 0 1.88 0.22 4 10 0 31.54 0.48 5 10 0 45.35 0.54 6 10 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